HPLC method for detecting methylsulfonyl chloride content in industrial waste liquid
A technology of methanesulfonyl chloride and methanesulfonyl chloride solution, which is applied in the field of chemical analysis, can solve the problems of no liquid chromatography detection method for methanesulfonyl chloride, no ultraviolet absorption functional group, and low content of methanesulfonyl chloride. Achieve the effect of good stability, accurate sensitivity and high recovery rate
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Embodiment 1
[0030] Instruments and Conditions:
[0031] Liquid chromatograph: Agilent 1260HPLC
[0032] Chromatographic column: Waters XBridge C18 (150mm*4.6mm, 3.5um)
[0033] Column temperature: 35°C
[0034] Mobile phase A: 0.05% trifluoroacetic acid in water (v / v)
[0035] Mobile phase B: 0.05% trifluoroacetic acid in acetonitrile (v / v)
[0036] Flow rate: 1.0ml / min
[0037] Injection volume: 2μL
[0038] Wavelength: 210nm;
[0039] The elution gradient is as follows:
[0040] Time(min)
A％
B％
-
95
5
5.0
40
60
7.0
10
90
9.0
10
90
10.0
95
5
15.0
95
5
[0041] Experimental steps:
[0042] Diluent: Acetonitrile.
[0043] Derivatization reagent: 5% benzylamine in acetonitrile.
[0044] Standard methanesulfonyl chloride solution: Weigh about 50mg of methanesulfonyl chloride into a 50mL volumetric flask containing 10ml of diluent, add diluent to volume and shake well, precisely pipette 1mL o...
Embodiment 2
[0047] Example 2: Methodological Validation
[0048] 1. Exclusive experiment
[0049] Take an appropriate amount of methylsulfonyl chloride reference substance, prepare a standard methylsulfonyl chloride solution according to the method of Example 1, and detect and analyze the solution by liquid chromatography according to the method of Example 1.
[0050] The experimental results show that at the retention time of methanesulfonyl chloride, there is no interference from the blank; the tailing factor of methanesulfonyl chloride is 0.9, and the peak shape is good; the separation between methanesulfonyl chloride and its adjacent peaks is 1.5, which is good. see details Figure 4 .
[0051] 2. Quantitation limit experiment
[0052] Take an appropriate amount of methylsulfonyl chloride reference substance, prepare a standard methylsulfonyl chloride solution according to the method of Example 1, and detect and analyze the solution by liquid chromatography according to the method ...
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